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Intrinsic flame-retardant modified natural rubber and preparation method thereof

A technology of natural rubber and intrinsic flame retardant, which is applied in the field of intrinsic flame retardant modified natural rubber and its preparation, and can solve the problems of adding large flame retardants, etc.

Active Publication Date: 2021-12-10
江苏北化新橡新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The invention provides an intrinsically flame-retardant modified natural rubber and a preparation method thereof, which are used to solve the problem that a large amount of flame retardants need to be added to traditional natural rubber for flame retardancy

Method used

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  • Intrinsic flame-retardant modified natural rubber and preparation method thereof
  • Intrinsic flame-retardant modified natural rubber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Epoxidized natural rubber (epoxy value 25%) was plasticized on an open mill for 5 minutes, and the distance between the rollers was 1mm. Take 5g of plasticized epoxidized natural rubber and dissolve it in 100mL of toluene. After complete dissolution, 12.6 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 0.2 g of triphenylphosphine were added and reacted for 4 hours under reflux condensation. The reaction temperature is 120° C., and the stirring speed is 200 r / min. Afterwards, 2.9 g of 4-amino-1,2,4-triazole and 0.05 g of triethylamine were added, and reacted for 2 hours under the condition of reflux condensation, the reaction temperature was 100° C., and the stirring speed was 200 r / min. After the reaction is finished, the prepared modified natural rubber is flocculated with methanol, washed and dried to obtain intrinsic flame-retardant modified natural rubber.

Embodiment 2

[0025] Epoxidized natural rubber (45% epoxy value) was plasticized on an open mill for 5 minutes, and the distance between the rollers was 1mm. Take 5g of plasticized epoxidized natural rubber and dissolve it in 100mL of chloroform. Add 10.4 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 0.4 g of triphenylphosphine, under the condition of reflux condensation, the reaction temperature is 130 ° C, and the The rotating speed is 250r / min, and the reaction time is 4 hours. After that, continue to add 2.3g of 5-amino-tetrazole and 0.1g of 2-ethyl-4-methylimidazole, under the condition of reflux condensation, the reaction temperature is 110°C, the stirring speed is 250r / min, and the reaction time is 1.5 hours . After the reaction is finished, the prepared modified natural rubber is flocculated with methanol, washed and dried to obtain intrinsic flame-retardant modified natural rubber.

Embodiment 3

[0027] Epoxidized natural rubber (50% epoxy value) was plasticized on an open mill for 5 minutes, and the distance between the rollers was 1 mm. Take 5g of plasticized epoxidized natural rubber and dissolve it in 100mL of dichloromethane. Add 12g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 0.3g of triphenylphosphine. 300r / min, the reaction time is 3 hours. Then, continue to add 2.8 g of 5-amino-tetrazole and 0.15 g of 2-methylimidazole. Under the condition of reflux condensation, the reaction temperature is 120° C., the stirring speed is 300 r / min, and the reaction time is 2 hours. After the reaction is finished, the prepared modified natural rubber is flocculated with methanol, washed and dried to obtain intrinsic flame-retardant modified natural rubber.

[0028] Above-mentioned each embodiment has measured the epoxy value before and after reaction by epoxy titration, calculates reaction conversion rate; Simultaneously, through vulcanization cross-linki...

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Abstract

The invention discloses an intrinsic flame-retardant modified natural rubber and a preparation method thereof. An epoxy group of a side chain of epoxidized natural rubber is used as a reaction active point, and the natural rubber of which the side chain is provided with triazole and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) is prepared by controlling reaction conditions and a material ratio. Compared with unmodified natural rubber, nitrogen-containing and phosphorus-containing functional groups are simultaneously introduced into the structure of the modified natural rubber, so that the modified natural rubber not only has better intrinsic flame retardant property, but also basically keeps the original physical and mechanical properties of the natural rubber. According to the intrinsic flame-retardant modified natural rubber prepared by the invention, on the premise of ensuring the flame retardant property, the dosage of the flame retardant in a composite material system can be reduced, the loss of the flame retardant on the mechanical property and the fatigue property of a composite material is reduced, and the intrinsic flame-retardant modified natural rubber has a very good application prospect in the field of intrinsic flame-retardant materials.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant polymer materials, and in particular relates to an intrinsic flame-retardant modified natural rubber and a preparation method thereof. Background technique [0002] Natural rubber (NR) has high elasticity, low internal friction, excellent mechanical properties, wear resistance, and bending fatigue resistance. It is one of the most widely used rubber varieties at present, and is widely used in tires, hoses, tapes and various rubber industries. products. Epoxidized natural rubber (ENR) is a high-performance rubber obtained by epoxidizing natural rubber. It is mainly prepared by reacting natural latex with peroxyacid, which improves the wet skid resistance and oil resistance of NR. , air tightness, bonding performance. Both natural rubber and epoxidized natural rubber have a structure with a carbon chain as the main chain, which is extremely flammable, and the heat release rate and smoke de...

Claims

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Application Information

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IPC IPC(8): C08C19/24C08C19/22
CPCC08C19/24C08C19/22
Inventor 杨建刘力李红霞储俊峰
Owner 江苏北化新橡新材料科技有限公司